CN101519434A - Extraction process of nosiheptide raw powder - Google Patents
Extraction process of nosiheptide raw powder Download PDFInfo
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- CN101519434A CN101519434A CN200910116488A CN200910116488A CN101519434A CN 101519434 A CN101519434 A CN 101519434A CN 200910116488 A CN200910116488 A CN 200910116488A CN 200910116488 A CN200910116488 A CN 200910116488A CN 101519434 A CN101519434 A CN 101519434A
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Abstract
The invention discloses an extraction process of nosiheptide raw powder. The original method using a centrifuge to separate zymotic fluid is changed to use a sheet frame to filter, thus the handling capacity in unit time is greatly improved and the equipment investment is reduced; in a crude product crystallization step, a definite mass of water is added in nosiheptide when concentration is finished by utilizing the characteristic that the nosiheptide is not dissolved in water, therefore, not only the cost is not increased, but also the yield coefficient ( the current yield coefficient is about 60 percent, and the yield coefficient of the invention is over 75 percent) can be greatly improved; in a refining step, the original butanol extraction is changed into water rinse so as to achieve the purpose of purification; and the valence of the nosiheptide raw powder produced by an improved refining process can reach 920-980 microgrammes/microgram, therefore, not only the product content is greatly improved, but also the production cost is greatly lowered by changing solvent extraction into acid water rinse. The extraction process has the advantages of simple process, high yield coefficient, good quality, and the like, thereby having commercial production conditions.
Description
Technical field:
The invention belongs to field of biological pharmacy, relate to a kind of animal and use antibiotic extracting method, be specifically related to a kind of extracting method for preparing the former powder of sulfur-bearing polypeptide antibiotics nosiheptide.
Technical background:
Along with the continuous progress of human material progress and people to the deepening constantly of nature understanding, the human beings'health development more and more receives much concern, the safety problem of food is also just most important.Meat fish egg milk brings with feed fully, guarantee the relieved of " eating " and " drinking ", will guarantee the safety of fish meat, eggs and milk, and therefore, the safety of feed is most important.Feed safety is meant in feed should not contain hazardous and noxious substances or factor, at least should be in aquatic animal not residually accumulates then is detrimental to health and environment for human survival is constituted a threat to.Nosiheptide is exactly a kind of green additive agent for feeding that meets people's demand fully.
Nosiheptide (nosiheptide) has another name called nosiheptide (primofax), multhiomycin (multhiomycin).Molecular formula: C51H43N13012S6, molecular weight 1222.37 is fermentation engineering products.It is a kind of novel not residual in animal body fodder additives by the polypeptide that 12 amino acid and derivative thereof are formed, and it is a kind of feeding antibiotic of novel non-absorption.
Nosiheptide technological element of a product height, raw materials cost low (soybean cake powder, Semen Maydis powder etc.), extraction process is simple, lower (the oral LD of the toxicity of product own
5013060 milligrams/kg body weight, abdominal injection LD
504610 milligrams/kg body weight).Behind livestock and poultry, this product of aquatic product animal edible, do not have residually in the body, and can obviously promote growth of animal and improve efficiency of feed utilization to meet the requirement of green product.The former powder of nosiheptide has the high characteristics of content, can significantly save its transportation cost concerning the manufacturer of downstream.
Summary of the invention:
The object of the present invention is to provide the extracting method of the former powder of a kind of nosiheptide.
The objective of the invention is to realize that by following technique means the extracting method of the former powder of nosiheptide comprises the steps:
A, get the nosiheptide fermented liquid and be heated to 80-90 ℃, insulation added flocculating aids more than 30 minutes, filtered;
B, get the nosiheptide filter residue, add 95% above ethanol in the ratio of 1:1.2, temperature control 45-50 ℃, stir process is more than 30 minutes, and suction filtration gets ethanol extract;
Filter residue behind c, the suction filtration adds 70% ethanol again, and temperature control 45-50 ℃, stir process is more than 30 minutes, and after carrying out extracting processing the second time, suction filtration gets ethanol extract;
D, filter residue repeat c step operation, extract one time again, then three ethanol extracts are merged;
E, with 60-65 ℃ of ethanol extract temperature control, vacuum tightness 0.08-0.09Mpa concentrating under reduced pressure ethanol, dense when going out original volume 2/3rds liquid, stop to concentrate;
Add the purified water that is equivalent to 3 times of concentrated solution volumes in f, the concentrated solution, temperature is reduced to crystallization below 10 ℃, and is centrifugal, and 50-60 ℃ of drying gets nosipeptide crude product;
Purified water washing, the centrifugation of the pH value 2-3 that is equivalent to 10 times of its weight of g, nosipeptide crude product, and then with the washing of the purified water of pH value 8-9, centrifugation, separate the former powder of back nosiheptide and use washing with acetone again, centrifugation is drying to obtain the former powder of nosiheptide then.
Further technical scheme of the present invention is to filter in the above-mentioned a step to adopt Plate Filtration.
As seen from the above technical solution, the present invention original method with whizzer separate fermentation liquid, uses Plate Filtration instead aspect the fermented liquid centrifugation, improved the unit time treatment capacity so greatly, reduces facility investment; In crude product crystallization step, utilize the water-fast character of nosiheptide, when concentrating end, add a certain amount of water, neither increase cost, can increase substantially yield (present existing yield is about 60%, and yield of the present invention reaches more than 75%) again; Purification step is used acid rinsing instead by original butyl alcohol extraction, to reach the purpose of purification, the former powder of nosiheptide of the process for refining production after the improvement is tired and can be reached 920-980ug/mg, has not only increased substantially product content but also used acid rinsing instead by solvent extraction to reduce production costs significantly.It is simple that extraction process of the present invention has method, the yield height, and advantages such as quality better possess commercial production conditions.
Embodiment:
Embodiment one:
A, get nosiheptide fermented liquid 3500ml and be heated to 80 ℃, be incubated 35 minutes, add flocculating aids, Plate Filtration;
B, get the nosiheptide filter residue, add 95% above ethanol in the ratio of 1:1.2,45 ℃ of temperature controls, stir process 30 minutes, suction filtration gets ethanol extract;
Filter residue behind c, the suction filtration adds 70% ethanol again, 45 ℃ of temperature controls, and stir process 30 minutes, after carrying out extracting processing the second time, suction filtration gets ethanol extract;
D, filter residue repeat c step operation, extract one time again, then three ethanol extracts are merged 3470ml altogether;
E, with 60 ℃ of ethanol extract temperature controls, vacuum tightness 0.08Mpa concentrating under reduced pressure ethanol, dense when going out original volume 2/3rds liquid, stop to concentrate;
Add the purified water that is equivalent to 3 times of concentrated solution volumes in f, the concentrated solution, temperature is reduced to crystallization below 10 ℃, and is centrifugal, and 50 ℃ of dryings get nosipeptide crude product 7.18g;
Acid rinsing, the centrifugation of the pH value 2-3 that is equivalent to 10 times of its weight of g, nosipeptide crude product, and then with the washing of the purified water of pH value 8-9, centrifugation, separate the former powder of back nosiheptide and use washing with acetone again, centrifugation is drying to obtain the former powder 5.11g of nosiheptide then.
The fermented liquid 3500ml 1800ug/ml total 100,000,000 that tires
Ethanol extract 3470ml total 100,000,000 yields 96.51% of 1752ug/ml of tiring
Crude product 7.18g total 100,000,000 yields 90.63% of 767ug/mg of tiring
Smart powder 5.11g total 100,000,000 yields 87.90% of 948ug/mg of tiring
Total recovery: 0.0484 ÷, 0.063 * 100%=76.83%
Embodiment two:
A, get nosiheptide fermented liquid 15000ml and be heated to 85 ℃, be incubated 30 minutes, add flocculating aids, Plate Filtration;
B, get the nosiheptide filter residue, add 95% above ethanol in the ratio of 1:1.2,48 ℃ of temperature controls, stir process 35 minutes, suction filtration gets ethanol extract;
Filter residue behind c, the suction filtration adds 70% ethanol again, 45 ℃ of temperature controls, and stir process 35 minutes, after carrying out extracting processing the second time, suction filtration gets ethanol extract;
D, filter residue repeat c step operation, extract one time again, then three ethanol extracts are merged 14350ml altogether;
E, with 55 ℃ of ethanol extract temperature controls, vacuum tightness 0.09Mpa concentrating under reduced pressure ethanol, dense when going out original volume 2/3rds liquid, stop to concentrate;
Add the purified water that is equivalent to 3 times of concentrated solution volumes in f, the concentrated solution, temperature is reduced to crystallization below 10 ℃, and is centrifugal, and 55 ℃ of dryings get nosipeptide crude product 26.85g;
Acid rinsing, the centrifugation of the pH value 2-3 that is equivalent to 10 times of its weight of g, nosipeptide crude product, and then with the washing of the purified water of pH value 8-9, centrifugation, separate the former powder of back nosiheptide and use washing with acetone again, centrifugation is drying to obtain the former powder 20.41g of nosiheptide then.
The fermented liquid 15000ml 1685ug/ml total 100,000,000 that tires
Ethanol extract 14350ml total 100,000,000 yields 95.65% of 1686ug/ml of tiring
Crude product 26.85g total 100,000,000 yields 92.98% of 838ug/mg of tiring
Smart powder 20.41g total 100,000,000 yields 88.44% of 975ug/mg of tiring
Total recovery: 0.199 ÷, 0.253 * 100%=78.66%
Embodiment three:
A, get nosiheptide fermented liquid 8000ml and be heated to 90 ℃, be incubated 30 minutes, add flocculating aids, Plate Filtration;
B, get the nosiheptide filter residue, add 95% above ethanol in the ratio of 1:1.2,50 ℃ of temperature controls, stir process 30 minutes, suction filtration gets ethanol extract;
Filter residue behind c, the suction filtration adds 70% ethanol again, 50 ℃ of temperature controls, and stir process 30 minutes, after carrying out extracting processing the second time, suction filtration gets ethanol extract;
D, filter residue repeat c step operation, extract one time again, then three ethanol extracts are merged 7470ml altogether;
E, with 65 ℃ of ethanol extract temperature controls, vacuum tightness 0.08Mpa concentrating under reduced pressure ethanol, dense when going out original volume 2/3rds liquid, stop to concentrate;
Add the purified water that is equivalent to 3 times of concentrated solution volumes in f, the concentrated solution, temperature is reduced to crystallization below 10 ℃, and is centrifugal, and 60 ℃ of dryings get nosipeptide crude product 15.03g;
Acid rinsing, the centrifugation of the pH value 2-3 that is equivalent to 10 times of its weight of g, nosipeptide crude product, and then with the washing of the purified water of pH value 8-9, centrifugation, separate the former powder of back nosiheptide and use washing with acetone again, centrifugation is drying to obtain the former powder 11.79g of nosiheptide then.
The fermented liquid 8000ml 1750ug/ml total 100,000,000 that tires
Ethanol extract 7470ml total 100,000,000 yields 94.29% of 1763ug/ml of tiring
Crude product 15.03g total 100,000,000 yields 93.94% of 825ug/mg of tiring
Smart powder 11.79g total 100,000,000 yields 92.74% of 975ug/mg of tiring
Total recovery: 0.115 ÷, 0.14 * 100%=82.1%
Claims (2)
1, the extracting method of the former powder of nosiheptide is characterized in that:
A, get the nosiheptide fermented liquid and be heated to 80-90 ℃, insulation added flocculating aids more than 30 minutes, filtered;
B, get the nosiheptide filter residue, add 95% above ethanol in the ratio of 1:1.2, temperature control 45-50 ℃, stir process is more than 30 minutes, and suction filtration gets ethanol extract;
Filter residue behind c, the suction filtration adds 70% ethanol again, and temperature control 45-50 ℃, stir process is more than 30 minutes, and after carrying out extracting processing the second time, suction filtration gets ethanol extract;
D, filter residue repeat c step operation, extract one time again, then three ethanol extracts are merged;
E, with 60-65 ℃ of ethanol extract temperature control, vacuum tightness 0.08-0.09Mpa concentrating under reduced pressure ethanol, dense when going out original volume 2/3rds liquid, stop to concentrate;
Add the purified water that is equivalent to 3 times of concentrated solution volumes in f, the concentrated solution, temperature is reduced to crystallization below 10 ℃, and is centrifugal, and 50-60 ℃ of drying gets nosipeptide crude product;
Acid rinsing, the centrifugation of the pH value 2-3 that is equivalent to 10 times of its weight of g, nosipeptide crude product, and then with the washing of the purified water of pH value 8-9, centrifugation, separate the former powder of back nosiheptide and use washing with acetone again, centrifugation is drying to obtain the former powder of nosiheptide then.
2, the extracting method of the former powder of nosiheptide according to claim 1 is characterized in that: filter in the described a step and adopt Plate Filtration.
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| CN200910116488A CN101519434A (en) | 2009-04-03 | 2009-04-03 | Extraction process of nosiheptide raw powder |
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Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105198958A (en) * | 2015-09-29 | 2015-12-30 | 浙江汇能动物药品有限公司 | Nosiheptide finemeal extracting method |
| CN105420319A (en) * | 2015-12-24 | 2016-03-23 | 山东胜利生物工程有限公司 | Preparation method of pure nosiheptide |
| CN106083995A (en) * | 2016-08-26 | 2016-11-09 | 宁夏泰益欣生物科技有限公司 | A kind of extracting method of nosiheptide |
| CN106317173A (en) * | 2016-08-23 | 2017-01-11 | 宁夏泰瑞制药股份有限公司 | Method for preparing coarse nosiheptide product by utilizing nosiheptide fermentation liquor |
| CN106317174A (en) * | 2016-08-25 | 2017-01-11 | 宁夏泰益欣生物科技有限公司 | Preparing method of crude nosipeptide |
| CN106560474A (en) * | 2015-12-06 | 2017-04-12 | 宁夏际华环境安全科技有限公司 | Production process for nosiheptide |
| CN109060980A (en) * | 2018-08-07 | 2018-12-21 | 河北圣雪大成制药有限责任公司 | A method of Nosiheptide content in detection Nosiheptide fermentation liquid |
| CN109467587A (en) * | 2018-11-27 | 2019-03-15 | 河北圣雪大成制药有限责任公司 | A method of improving Nosiheptide fermentation liquid filtering velocity |
| CN109796520A (en) * | 2019-02-20 | 2019-05-24 | 山东齐发药业有限公司 | A kind of extracting method of Nosiheptide fine work |
-
2009
- 2009-04-03 CN CN200910116488A patent/CN101519434A/en active Pending
Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105198958A (en) * | 2015-09-29 | 2015-12-30 | 浙江汇能动物药品有限公司 | Nosiheptide finemeal extracting method |
| CN106560474A (en) * | 2015-12-06 | 2017-04-12 | 宁夏际华环境安全科技有限公司 | Production process for nosiheptide |
| CN105420319A (en) * | 2015-12-24 | 2016-03-23 | 山东胜利生物工程有限公司 | Preparation method of pure nosiheptide |
| CN106317173A (en) * | 2016-08-23 | 2017-01-11 | 宁夏泰瑞制药股份有限公司 | Method for preparing coarse nosiheptide product by utilizing nosiheptide fermentation liquor |
| CN106317174A (en) * | 2016-08-25 | 2017-01-11 | 宁夏泰益欣生物科技有限公司 | Preparing method of crude nosipeptide |
| CN106083995A (en) * | 2016-08-26 | 2016-11-09 | 宁夏泰益欣生物科技有限公司 | A kind of extracting method of nosiheptide |
| CN109060980A (en) * | 2018-08-07 | 2018-12-21 | 河北圣雪大成制药有限责任公司 | A method of Nosiheptide content in detection Nosiheptide fermentation liquid |
| CN109467587A (en) * | 2018-11-27 | 2019-03-15 | 河北圣雪大成制药有限责任公司 | A method of improving Nosiheptide fermentation liquid filtering velocity |
| CN109796520A (en) * | 2019-02-20 | 2019-05-24 | 山东齐发药业有限公司 | A kind of extracting method of Nosiheptide fine work |
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Application publication date: 20090902 |